CN107473265A - A kind of method of powder body material cladding titanium dioxide - Google Patents
A kind of method of powder body material cladding titanium dioxide Download PDFInfo
- Publication number
- CN107473265A CN107473265A CN201710744394.5A CN201710744394A CN107473265A CN 107473265 A CN107473265 A CN 107473265A CN 201710744394 A CN201710744394 A CN 201710744394A CN 107473265 A CN107473265 A CN 107473265A
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- China
- Prior art keywords
- body material
- powder body
- titanium dioxide
- powder
- calcining
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
Abstract
The present invention proposes a kind of method of powder body material cladding titanium dioxide.Comprise the following steps：Powder body material is stirred into certain time under conditions of certain air humidity is；Test is taken out after reaching certain moisture content to powder body material；Powder body material is added to titanium salt solution immersion under nitrogen protective condition, terminated to hydrolysis；Then dried after powder body material is filtered；Dried powder body material is finally calcined into certain time again, the coated by titanium dioxide layer of anatase titanium dioxide or rutile-type can be obtained by temperature difference.The utilization rate of titanium salt of the present invention greatly increases, and ensure only to control the phenomenon that difficult, titanium salt utilization rate is low, is mingled with titanium dioxide in product in the coated with uniform layer of titanium dioxide of powder body material so as to reduce covered effect caused by usual powder body material coats under the conditions of titanium salt colloidal sol etc..
Description
Technical field
The invention belongs to field of material preparation, is related to powder body material coating technology, specifically on a kind of powder body material bag
Cover the method for titanium dioxide.
Background technology
Single-phase powder body material is often because the limitation of some structures and performance so that its application effect to a certain extent by
To influence.Therefore, the surface modification of powder, surface modification or even the phase structure and property that change material using surface coating technology
Research developed.In recent years, these aspects, especially in terms of the preparation and application of cell positive material, nano material,
Achieve very big development.
The surface modification of powder is that solve a kind of most important approach that superfine powder is reunited, surface is modified.The table of powder
Face modification mainly improves the surface chemistry and physical characteristic of powder, is improving powder dispersiveness in media as well, is reducing powder
Reunion degree, chemical property etc. while, assign material new characteristic.
It is existing to utilize titanium salt Hydrolyze method existing cladding residue when powder body material surface coats layer of titanium dioxide
Difficult, cladding homogeneity is poor, the problems such as titanium salt utilization rate is low.
The content of the invention
The present invention proposes a kind of method of powder body material cladding titanium dioxide, utilizes powder to solve above technical problem
Material surface moisture film and titanium salt solution haptoreaction, it is mingled with the mesh of titanium dioxide so as to reach coated with uniform and not produce
's.
The technical solution adopted by the present invention is：A kind of method of powder body material cladding titanium dioxide, comprises the following steps：
1）Stirred under conditions of being 60%~100% in air humidity by powder body material；
2）Test is taken out to powder body material moisture content after being 10~60% when powder body material moisture content in whipping process；
3）By 2）In powder body material added under nitrogen protective condition titanium salt solution immersion, terminate to hydrolysis, mixed
Close slurries；
4）By 3）Middle mixed serum filtering, obtains filtering powder, dries filter powder；
5）By 4）In dried filter powder calcining, control calcining heat, obtain the coated by titanium dioxide of anatase titanium dioxide or rutile-type
Layer.
Further, the solute in described titanium salt solution is the titanium salt that hydrolysis can occur, and is titanium tetrachloride, metatitanic acid
One kind in four butyl esters, tetraethyl titanate, isopropyl titanate.
Further, drying mode used is fluidized bed drying, expansion drying, tray drying, microwave when drying filter powder
Dry one kind；Drying temperature is 50~300 DEG C.
Further, the calcining manners used during calcining filter powder is dynamic calcining or Static Calcinations, or above two calcining
The combination of method；Calcining heat is 500~900 DEG C；Calcination time is 1~8h.
Further, calcining filter powder procedure regulation atmosphere oxygen content, atmosphere oxygen content are 21%~80%.
The present invention has the advantages that compared with the prior art：
The characteristics of hydrolysis directly occurs, powder body material table after the pre-treatment are contacted with water present invention utilizes titanium salt solution
Direct hydrolysis reaction on the moisture film that face is formed, then unnecessary titanium salt solution is filtered；Then powder body material is subjected to calcination processing,
Form fine and close, uniform coated by titanium dioxide film.
Being mainly characterized by of the technology by the pretreatment to powder body material, define titanium salt solution hydrolysis position and
Film thickness, effectively solve the validity and amount of titanium salt cladding so as to succinct, and do not produce the unnecessary titanium dioxide that is mingled with,
It ensure that the uniformity and uniformity of powder body material after coating.This method is succinctly efficient, considerably increases utilization rate, the bag of titanium salt
The uniformity covered, the titanium dioxide eliminated in material are mingled with, and improve covered effect.
Brief description of the drawings
Fig. 1 is the powder body material electron microscope after present invention cladding.
Embodiment
Embodiment 1
1）100g cobalt acid lithiums are put into humidistat, stirred 1 hour under conditions of being 80% in humidity；
2）Sampling and testing to powder body material moisture content takes out after being 10%；
3）By 2）In cobalt acid lithium be put into atmosphere reactor, under nitrogen protective condition add titanium tetrachloride solution 500ml, leaching
Bubble 2 hours, obtains mixed serum；
4）By 3）In mixed serum filtered with filter press, obtain filter powder；
5）Filter powder after filtering is put into fluidized bed drying, 200 DEG C of drying temperature；
6）By 5）In it is dried filter powder 700 DEG C calcine 2 hours, you can obtain anatase titanium dioxide clad cobalt acid
Lithium.
As can be seen that the obtained coating product of this method is uniform in Fig. 1, without being mingled with.
Embodiment 2
1）100g nickle cobalt lithium manganates are put into humidistat, stirred 2 hours under conditions of being 50% in humidity；
2）Sampling and testing to powder body material moisture content takes out after being 20%；
3）By 2）In nickle cobalt lithium manganate be put into atmosphere reactor, add titanium tetrachloride solution under nitrogen protective condition
100ml, soak 1 hour, obtain mixed serum；
4）By 3）In mixed serum filtered with filter press, obtain filter powder；
5）Filter powder after filtering is put into vacuum drying chamber to dry, 150 DEG C of drying temperature；
6）By 5）In it is dried filter powder 850 DEG C calcine 3 hours, you can obtain rutile titanium dioxide clad cobalt manganese
Sour lithium.
The present invention is hydrolyzed and forged again after particularly first being pre-processed to powder body material using the characteristic of titanium salt hydrolysis
Burn.So that greatly increased to the utilization rate of titanium salt, and ensure only in the coated with uniform layer of titanium dioxide of powder body material, from
And reduce caused by usual powder body material is coated under the conditions of titanium salt colloidal sol etc. covered effect control is difficult, titanium salt utilization rate is low,
It is mingled with the phenomenon of titanium dioxide in product.
Although the preferred embodiments of the present invention are described above, the invention is not restricted to above-mentioned specific embodiment party
Formula, above-mentioned embodiment are only exemplary rather than limited, and one of ordinary skill in the art is in the present invention
Enlightenment under, on the premise of without prejudice to present inventive concept and claim, expression, such change as multiple types can be made
Change and each fall within protection scope of the present invention.
Claims (5)
- A kind of 1. method of powder body material cladding titanium dioxide, it is characterised in that comprise the following steps：1）Stirred under conditions of being 60%~100% in air humidity by powder body material；2）Test is taken out to powder body material moisture content after being 10~60% when powder body material moisture content in whipping process；3）By 2）In powder body material added under nitrogen protective condition titanium salt solution immersion, terminate to hydrolysis, mixed Close slurries；4）By 3）Middle mixed serum filtering, obtains filtering powder, dries filter powder；5）By 4）In dried filter powder calcining, control calcining heat, obtain the coated by titanium dioxide of anatase titanium dioxide or rutile-type Layer.
- 2. the method for powder body material cladding titanium dioxide according to claim 1, it is characterised in that：Described titanium salt solution In solute be the titanium salt that hydrolysis can occur, be titanium tetrachloride, butyl titanate, tetraethyl titanate, in isopropyl titanate It is a kind of.
- 3. the method for powder body material cladding titanium dioxide according to claim 1, it is characterised in that：Dry used during filter powder Drying mode for fluidized bed drying, expansion drying, tray drying, one kind of microwave drying；Drying temperature is 50~300 DEG C.
- 4. the method for powder body material cladding titanium dioxide according to claim 1, it is characterised in that：Used during calcining filter powder Calcining manners be dynamic calcining or Static Calcination, or the combination of above two method for calcinating；Calcining heat is 500~900 DEG C； Calcination time is 1~8h.
- 5. the method for powder body material cladding titanium dioxide according to claim 4, it is characterised in that：Calcining filter powder process is adjusted Solar term atmosphere oxygen content, atmosphere oxygen content are 21%~80%.
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| CN201710744394.5A CN107473265B (en) | 2017-08-25 | 2017-08-25 | A kind of method of powder body material cladding titanium dioxide |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005119820A1 (en) * | 2004-06-01 | 2005-12-15 | Vk Corporation | Positive electrode active material for lithium ion secondary cell coated hetero metal oxide on the surface and lithium ion secondary cell comprising it |
| CN102315430A (en) * | 2011-10-21 | 2012-01-11 | 佛山市邦普循环科技有限公司 | Preparation method for metallic oxide cladded anode material of lithium ion battery |
| CN104319396A (en) * | 2014-09-19 | 2015-01-28 | 青岛乾运高科新材料股份有限公司 | Preparation method of surface cladding material of lithium ion battery cathode material |
| CN104617267A (en) * | 2015-01-21 | 2015-05-13 | 长沙矿冶研究院有限责任公司 | Ultrathin TiO2 coating layer of lithium battery cathode material, lithium battery cathode material and preparation method of lithium battery cathode material |
-
2017
- 2017-08-25 CN CN201710744394.5A patent/CN107473265B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005119820A1 (en) * | 2004-06-01 | 2005-12-15 | Vk Corporation | Positive electrode active material for lithium ion secondary cell coated hetero metal oxide on the surface and lithium ion secondary cell comprising it |
| CN102315430A (en) * | 2011-10-21 | 2012-01-11 | 佛山市邦普循环科技有限公司 | Preparation method for metallic oxide cladded anode material of lithium ion battery |
| CN104319396A (en) * | 2014-09-19 | 2015-01-28 | 青岛乾运高科新材料股份有限公司 | Preparation method of surface cladding material of lithium ion battery cathode material |
| CN104617267A (en) * | 2015-01-21 | 2015-05-13 | 长沙矿冶研究院有限责任公司 | Ultrathin TiO2 coating layer of lithium battery cathode material, lithium battery cathode material and preparation method of lithium battery cathode material |
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| CN107473265B (en) | 2019-04-26 |
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